Determination of Particle Size Distribution Parameters using a Laser-Scattered Light Spectrometer

A method based on the measurement of scattered light intensity distributions is demonstrated to be able to determine directly the particle size of monodisperse supermicron-size particles. In all other cases of a particle cloud, information about the size distribution can be acquired from comparison of measured and calculated intensities as a function of scattering angle. This indirect method is only applicable if the assumptions made in the theory used for comparison are fulfilled. Therefore, the method is limited to spherical particles with known refractive index. The type of size distribution also has to be known. In the cases considered a log-normal size distribution was assumed. The uncertainty of the result increases with increase in the number of parameters that have to be determined. The method seems to be limited to unimodal distributions described with two parameters.     

Size and Shape Prediction of Colloidal Metal Oxide MgBaFeO Particles from Light Scattering Measurements

The size and structure of colloidal metal oxide (MgBaFeO) particles are determined using an Elliptically Polarized Light Scattering (EPLS) technique. The approach is based on a hybrid experimental/theoretical study where the experimental data are compared against predictions obtained using a T-Matrix model that accounts for particle shape irregularities. A power-law distribution function with two parameters is employed to account for the particle size distribution. The refractive index of the particles in ethyl alcohol is calculated based on the Maxwell-Garnet formula. The experiments are conducted using a second-generation nephelometer. It is shown that the current EPLS measurements can effectively be used for identification of both the shape and the size of the colloids.     

Rationale and principle of an instrument measuring lung deposited nanoparticle surface area

The risk of nanoparticles by inhalation for human health is still being debated but some evidences of risk on specific properties of particles <100 nm diameter exist. One of the nanoparticle parameters discussed by toxicologists is their surface area concentration as a relevant property for e.g. causing inflammation. Concentrations of these small particles (~ <100 nm) are currently not measured, since the mass concentrations of these small particles are normally low despite large surface area concentrations. Airborne particles will always be polydisperse and show a size distribution. Size is normally described by an equivalent diameter to include deviations in properties from ideal spherical particles. Here only nanoparticles below a certain size to be defined are of interest. Total concentration measures are determined by integration over the size range of interest. The ideal instrument should measure the particles according to the size weighting of the wanted quantity. Besides for the geometric surface area the wanted response function can be derived for the lung deposited surface area in the alveolar region. This can be obtained by weighting the geometric surface area as a function of particle size with the deposition efficiency for the alveolar region for e.g. a reference worker for work place exposure determination. The investigation of the performance of an Electrical Aerosol Detector (EAD) for nearly spherical particles showed that its response function is close to the lung deposited surface areas in different regions of the human respiratory system. By changing the ion trap voltage an even better agreement has been achieved. By determining the size dependent response of the instrument as a function of ion trap voltage the operating parameters can be optimized to give the smallest error possible. Since the concept of the instrument is based on spherical particles and idealized lung deposition curves have been used, in all other cases errors will occur, which still have to be defined. A method is now available which allows in principle the determination of the total deposited surface area in different regions of the lung in real time. It can easily be changed from one deposited region to another by varying the ion trap voltage. It has the potential to become a routine measurement technique for area measurements and personal control in e.g. work place environments.     

Characterization of Sub‐Micron Perovskite Suspensions Formed Through Cavitation Processing

The size distribution within and electrokinetic properties of aqueous perovskite (LaCoO₃) suspensions, have been characterized as a function of processing conditions. Submicron–sized perovskite particles have been obtained using a cavitation technique in which the suspension is passed through a series of small orifices under extreme driving pressure drops. When no additives were used, the zeta potential of the particles was found to be positive over the entire pH range studied. Use of an acrylic copolymer surfactant with multiple negatively charged sites during the cavitation processing was found to improve dispersion stability. The observed variations in zeta potential and particle size for the suspensions are explained in terms of electrostatic interactions between particles, the tendency for the surfactant to adsorb onto the particles, and the degree of steric stabilization provided by the surfactant.     

The Measurement of Particles Suspended in a stirred vessel using microphotography and digital image analysis

A novel technique to determine the size of particles suspended in a stirred vessel is investigated. The method uses microphotography to obtain a still image of the particles in situ. The equivalent circular diameter of the particles is obtained from the photographs using digital image analysis. The particles used for the test were certified particle size standards of a very small tolerance in diameter deviation. The size comparison was determined as a percent error between the measured particle diameter (equivalent circular diameter) and the diameter established by the particle manufacturer. To determine the limiting ranges of particle size and concentrations, spherical particles in a size range of approximately 1 to 10.0 μm (microns) in diameter were employed in the test. Concentrations varied from 0.00005% to 0.1% (mass basis). For each particle size, an aqueous solution of the particles was prepared at the desired concentration and placed in a stirred vessel. Photographs of the solutions were made at 25.5x, 40x, 60x and 80x magnification. For all sizes of particles, the entire range of concentration was examined. The results indicate a minimum size resolution of approximately 3μm, in a corresponding concentration range of 0.0001% to 0.05%. Similar limits on concentration were found for the larger diameter particles, although a true upper limit for the largest particle sizes was not established. The functional concentration range appears to shift towards higher mass concentrations with increasing particle size. For 2.92 μm diameter particles, the error in size measurement was found to be below 10% for a concentration range of 0.0005% to 0.05%. Additionally, a relationship between turbidity and the error was seen at low particle concentration levels where decreasing levels of turbidity generated increasing levels of error.     

双峰分布颗粒体系的多角度动态光散射数据反演

采用多角度动态光散射和加权正则化反演方法,对4组模拟的双峰分布颗粒体系(100/600 nm,200/600 nm,300/600 nm和350/600 nm)分别选取1、3、6和10个散射角进行测量.粒度反演结果表明,采用加权正则化方法反演双峰颗粒体系的多角度动态光散射测量数据,可获得峰值位置比小于2∶1且含有大粒径(＞350 nm)颗粒的双峰颗粒粒度分布.采用标准聚苯乙烯乳胶颗粒进行实测的结果验证了这一结论.得到含大粒径颗粒的双峰粒度分布反演结果的原因在于,多角度动态光散射能提供更多的大粒径颗粒的粒度信息,加权正则化反演方法能减少测量数据中的噪声,因而多角度动态光散射测量数据的加权反演能实现峰值位置比小于2∶1且含有大粒径颗粒的双峰颗粒体系的测量.     

Modelling study on the three-dimensional neutron depolarisation response of the evolving ferrite particle size distribution during the austenite–ferrite phase transformation in steels

The magnetic configuration of a ferromagnetic system with mono-disperse and poly-disperse distribution of magnetic particles with inter-particle interactions has been computed. The analysis is general in nature and applies to all systems containing magnetically interacting particles in a non-magnetic matrix, but has been applied to steel microstructures, consisting of a paramagnetic austenite phase and a ferromagnetic ferrite phase, as formed during the austenite-to-ferrite phase transformation in low-alloyed steels. The characteristics of the computational microstructures are linked to the correlation function and determinant of depolarisation matrix, which can be experimentally obtained in three-dimensional neutron depolarisation (3DND). By tuning the parameters in the model used to generate the microstructure, we studied the effect of the (magnetic) particle size distribution on the 3DND parameters. It is found that the magnetic particle size derived from 3DND data matches the microstructural grain size over a wide range of volume fractions and grain size distributions. A relationship between the correlation function and the relative width of the particle size distribution was proposed to accurately account for the width of the size distribution. This evaluation shows that 3DND experiments can provide unique in situ information on the austenite-to-ferrite phase transformation in steels.     

Study of the mobility,surface area,and sintering behavior of agglomerates in the transition regime by tandem differential mobility analysis

The surface area of nanosized agglomerates is of great importance as the reactivity and health effects of such particles are highly dependent on surface area. Changes in surface area through sintering during nanoparticle synthesis processes are also of interest for precision control of synthesised particles. Unfortunately, information on particle surface area and surface area dynamics is not readily obtainable through traditional particle mobility sizing techniques. In this study, we have experimentally determined the mobility diameter of transition regime agglomerates with 3, 4, and 5 primary particles. Agglomerates were produced by spray drying well-characterised polystyrene latex particles with diameters of 55, 67, 76, and 99 nm. Tandem differential mobility analysis was used to determine agglomerate mobility diameter by selecting monodisperse agglomerates with the same number of primary particles in the first DMA, and subsequently completely sintering the agglomerates in a furnace aerosol reactor. The size distribution of the completely sintered particles was measured by an SMPS system, which allowed for the determination of the number of primary particles in the agglomerates. A simple power law regression was used to express mobility diameter as a function of primary particle size and the number of primary particles, and had an excellent correlation (R² = 0.9971) with the experimental data. A scaling exponent was determined from the experimental data to relate measured mobility diameter to surface area for agglomerates. Using this relationship, the sintering characteristics of agglomerates were also examined for varying furnace temperatures and residence times. The sintering data agreed well with the geometric sintering model (GSM) model proposed by Cho & Biswas (2006a) as well as with the model proposed Koch & Friedlander (1990) for sintering by viscous flow.     

Locally Resolving Measurements of PSD,Particle Concentration and Particle Velocity by Means of TFS with Dual Beams

Transmission fluctuation spectrometry with spatial correlation (TFS‐SC) is based on transmitting two beams of radiation through a flowing suspension, whereby the distance of the beam centers is varied. Thus, the spatial correlation of the transmission fluctuations of the two beams is determined as a function of the beam distance. By numerical modeling, the transition functions of the correlation are found as a function of beam distance, beam diameters, particle diameter and beam intersection angle. Experimentally determined spatial correlation spectra can be inverted to obtain the particle concentration and particle size distribution by using the theoretical transition functions for mono‐sized particles. In addition, time correlations can be used to extract information on particle velocity. Some experimental results obtained by TFS‐SC are presented and discussed. This method appears promising for application in the local resolving of measurements of PSD, particle concentration and particle velocity in two‐phase flows, both in the laboratory and in process control.     

Scanning acoustic Doppler microscopy and scanning acoustic correlation microscopy

Acoustic microscopy with vector contrast at 100 MHz in a fluid with immersed particles is used to detect the flow profile in front of a microscopic orifice. The velocity profile concerning the component in axial direction of the focused beam is derived from the phase contrast. Possibilities to resolve the flow profile also for the components in normal direction with respect to the axis are demonstrated. The methods concerning measurement techniques and data evaluation for scanning acoustic Doppler microscopy are presented. For scanning acoustic correlation microscopy the time dependent phase and amplitude signals resulting from sound waves scattered by the immersed particles (aluminium flakes with a typical diameter of 10 microm) have been analysed by correlation procedures. From the obtained autocorrelation functions the velocity distribution can be derived. Both methods can be applied simultaneously. Data analysis is based on the information contained in the originally obtained images in vector contrast derived from temporal and spatial resolved analogue and digital processing of the acoustic signals.     

Deconvolution with Maximum Entropy Solution to Determine Local Extinction Coefficient and Local Volume Concentration Values from Laser Diffraction Data

The traditional use of the laser diffraction technique provides line‐of‐sight liquid spray drop‐size distribution. However, deconvolution of the measurements can be performed for axisymmetric spray in order to determine local spray characteristics. In a previous publication, a new deconvolution technique making use of the maximum entropy principle was established and applied to determine the local drop‐size distributions. The entire approach was experimentally validated. In this work, the technique is employed to determine local extinction coefficient values. As in the previous investigation, the measurement procedure consists of scanning a laser beam through the spray cross‐section from the center to the edge of the spray. By use of the transmittance theory, the local extinction coefficients allow the local volume concentrations to be calculated. This theory introduces the mean scattering coefficient. The results show that this coefficient must be determined as a function of the Sauter mean diameter in order to avoid overestimation of the volume concentration. Although no proper validation is presented, the coherence of the overall approach is discussed in detail and solutions for improving the spatial resolution are presented. Finally, the local volume concentrations are combined with the local drop‐size distribution to provide local volume‐weighted, drop‐size distributions. These distributions provide information on the localization of the drops according to their diameter as well as on the spatial liquid distribution. This work illustrates applications and performances of laser diffraction technique that are rarely used.     

Intercomparison of Inversion Algorithms for Particle‐Sizing Using Mie Scattering

The applicability of different inversion algorithms to retrieve a size distribution of particles in air from light scattering is examined. The investigation is focused on an optical measurement setup with an elliptical mirror as the main optical element. In order to evaluate the capabilities of the individual inversion methods, light scattering by spherical particles is simulated in the size ranges of 0.1 – 10 μm and 0.05 – 1 μm. The distribution of the particle diameters is modeled with three different parametric functions, i.e., RRSB, logarithmic‐normal and a more specific distribution from an ultrasonic nebulizer. Different kinds of noise, e.g., additive and/or multiplicative, are applied in different levels to the simulated scattering measurement to include real physical measurement conditions. The convergence properties of the scattering simulation are investigated with respect to the number of size classes, and thus, information concerning the size resolution required to simulate a measurement for a given particle size distribution is obtained. Further parameters of interest are the minimum angular resolution of the measurements, the number of size classes of the retrieved particle size distribution and the measured polarization of the scattered light.     

Simultaneous measurement of particle size, velocity, andtemperature in thermal plasmas

The in-flight measurement of particle parameters (size, velocity, temperature, and local number density) can prove insight into the plasma processing of solid materials. A measurement technique for simultaneously obtaining the size, velocity, and temperature of particles entrained in high-temperature flow fields is described. Particle size and velocity are obtained from a combination laser-particle-sizing system and laser Doppler velocimeter. The particle temperature is determined by a two-color pyrometry technique and the data rate is a measure of relative particle number density. Typical measured temperatures and velocities for the 5-100 μm particles used in plasma spraying are 1600-3500 K and 100-300 m/s, respectively. Since particle size, velocity, and temperature are measured simultaneously, cold particles (<1600 K) are identified and their relative number density can be quantified. Data from two plasma spray systems, a metal one (Ni-Al) and a metal oxide one (Al₂O₃), are presented and their application to understanding the plasma spray-coating process is illustrated     

Analysis of scattering medium structure from data on the multiple scattering of electromagnetic radiation

The radiation transfer equation for a semi -infinite scattering medium is solved. The solution provides information on the size distribution function of the scattering particles, starting from experimental data on the multiple scattering of electromagnetic radiation. A solution is obtained for the case where the probability of scattering is given by the solution of Mie's problem.     

Monte Carlo Simulations of Reflected Spectra Derived from Tissue Phantom with Double-Peak Particle Size Distribution

We made a tissue phantom with double-peak particle size distribution, which has polystyrene particles of cell nuclear size and mitochondrial size, and measured the spectrum from the tissue phantom using a single optical fiber. In this paper we investigate the characterization method for the tissue phantom with double-peak particle size distribution by comparing the measured spectra with the calculated ones using the Monte Carlo (MC) method. It is first shown that the Mie phase function characterizes better than the Henyey-Greenstein (H-G) phase function in MC calculation. Next, we compare the measurement spectra with those obtained by modeling as single-peak, conventional modeling for particle size distribution, and for double-peak particle size distribution. The single-peak modeling is found to cause considerable error for the tissue phantom with double-peak particle size distribution, which seems to simulate a biological tissue. We suggest that if one simulates the particle size distribution of a biological tissue by conventional modeling, the accuracy of estimation will be lower.     

Surface deposition and coagulation efficiency of combustion generated nanoparticles in the size range from 1 to 10 nm

The size distribution of the nanoparticles formed in premixed ethylene–air flames and collected thermophoretically on mica cleaved substrates is obtained by atomic force microscopy (AFM). The distribution function extends from 1 to about 5 nm in non-sooting flames and in the soot pre-inception region of the richer flames, while it becomes bimodal and larger particles are formed in the soot inception region of the slightly sooting flames. The distribution is compared with the size distribution of nano-sized organic carbon (NOC) and soot particles, obtained by “in situ” multi-wavelength extinction and light scattering methods. The deposition efficiency is estimated from the differences between these two size distribution functions as a function of the equivalent diameter of the nanoparticles. Furthermore, the coagulation coefficient of particles in flame is obtained from the temporal evolution of the number concentration of the nanoparticles inside the flames. NOC particles, which are rapidly produced in locally rich combustion regions, have peculiar properties since their sticking coefficient both for coagulation and adhesion result to be orders of magnitudes lower than that expected by larger aerosols, like soot particles. The experimental results are interpreted by modelling the van der Waals interactions of the nanoparticles in terms of Lennard-Jones potentials and in the framework of the gas kinetic theory. The estimated adhesion and coagulation efficiencies are in good agreement with those calculated from AFM and optical data. The very low efficiency values observed for the smaller particles could be ascribed to the high energy of these particles due to their Brownian motion, which causes thermal rebound effects prevailing over adhesion mechanisms due to van der Waals forces.     

Colloidal Analysis of Particles Extracted from Microalloyed Steels

Different colloidal particle characterization methods are examined for their suitability to determine the particle size distribution of particles extracted from steels. Microalloyed steels are dissolved to extract niobium and titanium carbonitride particles that are important for the mechanical properties of these steels. Such particles have sizes ranging from several nanometers to hundreds of nanometers depending on the precipitation stage during the thermomechanically controlled rolling process. The size distribution of the particles is analyzed by dynamic light scattering (DLS), analytical ultracentrifugation (AUC), and hollow fiber flow field-flow fractionation (HF5) and compared to data obtained for reference particles as well as data from electron microscopy, the standard sizing technique used in metallurgy today. AUC and HF5 provide high-quality size distributions, average over large particle numbers that enables statistical analysis, and yield useful insights for alloy design; however, DLS fails due to a lack of resolution. Important aspects in the conversion and comparison of size distributions obtained for broadly distributed particle systems with different measurement principles and the role of surfactants used in sample preparation are discussed.     

Comparison of PIV parameters effects on displacement identification and cross correlation

An algorithm is presented to determine displacements thanks to the identification method. Its main properties are described: no link with the particle size, measurement of the velocity distribution. Determination of effects of PIV parameters on displacement identification is made. Parameters used are noise, bias, velocity distribution. Therefore, we can define a validity domain of PIV parameters for identification and compare it with the domain of cross correlation. The identification validity range is based on 70% of isolated particles, on a displacement norm and on displacement gradients corresponding to less than half the size of the interrogation cell and to 10% of the average velocity. The comparison with cross correlation domains indicates that the cross correlation is more robust. However, the identification method is interesting because of the possibility of displacement distribution measurement. We use it to measure the decreasing of the turbulence intensity for a grid-generated turbulence.     

Soot particle size distributions in a well-stirred reactor/plug flow reactor

A well-stirred reactor (WSR) followed by a plug flow reactor (PFR) is being used to study polycyclic aromatic hydrocarbon (PAH) growth and soot inception. Soot size distributions were measured using a dilution probe followed by a nano-differential mobility analyzer (Nano-DMA). A rapid insertion probe was fabricated to thermophoretically collect particles from the reactor for transmission electron microscopy (TEM) imaging. Results are presented on the effect of equivalence ratio on the soot size distributions obtained for fixed dilution ratio, the effect of dilution ratio on the soot size distributions obtained for fixed equivalence ratio, and the effect of temperature on the soot size distributions obtained for fixed equivalence ratio. In addition to particle sizing measurements, gas samples were analyzed by a gas chromatograph to determine the concentration of gaseous species in the PFR thought to be important in soot formation. Our soot size distribution measurements demonstrate that the mixing conditions in the flame zone affect whether or not a nucleation mode was detected in the size distribution.